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--`,,``,,,,``,,``,`````,````,,-`-`,,`,,`,`,,`--- Designation: C 311 – 05

Standard Test Methods for


Sampling and Testing Fly Ash or Natural Pozzolans for Use
in Portland-Cement Concrete1
This standard is issued under the fixed designation C 311; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.

1. Scope 2. Referenced Documents


1.1 These test methods cover procedures for sampling and 2.1 ASTM Standards: 2
testing fly ash and raw or calcined pozzolans for use in C 33 Specification for Concrete Aggregates
portland-cement concrete. C 109/C 109M Test Method for Compressive Strength of
1.2 The procedures appear in the following order: Hydraulic Cement Mortars(Using 2-in. or [50-mm] Cube
Specimens)
Sections C 114 Test Methods for Chemical Analysis of Hydraulic
Sampling 7 Cement
CHEMICAL ANALYSIS
Reagents and apparatus 10
C 150 Specification for Portland Cement
Moisture content 11 and 12 C 151 Test Method for Autoclave Expansion of Hydraulic
Loss on ignition 13 and 14 Cement
Silicon dioxide, aluminum oxide, iron oxide, calcium oxide,
magnesium oxide, sulfur trioxide, sodium oxide C 157/C 157M Test Method for Length Change of Hard-
and potassium oxide 15 ened Hydraulic-Cement Mortar and Concrete
Available alkali 16 and 17 C 185 Test Method for Air Content of Hydraulic Cement
Ammonia 18
PHYSICAL TESTS Mortar
Density 19 C 188 Test Method for Density of Hydraulic Cement
Fineness 20 C 204 Test Methods for Fineness of Hydraulic Cement by
Increase of drying shrinkage of mortar bars 21-23
Soundness 24 Air-Permeability Apparatus
Air-entrainment of mortar 25 and 26 C 226 Specification for Air-Entraining Additions for Use in
Strength activity index with portland cement 27-30 the Manufacture of Air-Entraining Hydraulic Cement
Water requirement 31
Effectiveness of Fly Ash or Natural Pozzolan in C 227 Test Method for Potential Alkali Reactivity of
Controlling Alkali-Silica Reactions 32 Cement-Aggregate Combinations (Mortar-Bar Method)
Effectiveness of Fly Ash or Natural Pozzolan in C 430 Test Method for Fineness of Hydraulic Cement by
Contributing to Sulfate Resistance 34
the 45-µm (No. 325) Sieve
C 441 Test Method for Effectiveness of Pozzolans or
1.3 The values stated in SI units are to be regarded as the
Ground Blast-Furnace Slag in Preventing Excessive Expan-
standard. The values given in parentheses are provided for
sion of Concrete Due to the Alkali-Silica Reaction
information purposes only.
C 618 Specification for Coal Fly Ash and Raw or Calcined
1.4 This standard does not purport to address all of the
Natural Pozzolan for Use in Concrete
safety concerns, if any, associated with its use. It is the
C 670 Practice for Preparing Precision and Bias Statements
responsibility of the user of this standard to establish appro-
for Test Methods for Construction Materials
priate safety and health practices and determine the applica-
C 778 Specification for Sand
bility of regulatory limitations prior to use.
C 1012 Test Method for Length Change of Hydraulic-
1.5 The text of this standard references notes and footnotes
Cement Mortars Exposed to a Sulfate Solution
that provide explanatory information. These notes and foot-
C 1157 Performance Specification for Hydraulic Cement
notes (excluding those in tables) shall not be considered as
C 1437 Test Method for Flow of Hydraulic Cement Mortar
requirements of this standard.
D 1426 Test Methods for Ammonia Nitrogen In Water
1
These test methods are under the jurisdiction of ASTM Committee C09 on
2
Concrete and Concrete Aggregates and are the direct responsibility of Subcommit- For referenced ASTM standards, visit the ASTM website, www.astm.org, or
tee C09.24 on Supplementary Cementitious Materials. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved Dec. 15, 2005. Published January 2006. Originally Standards volume information, refer to the standard’s Document Summary page on
approved in 1953. Last previous edition approved in 2004 as C 311 – 04. the ASTM website.

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C 311 – 05
D 4326 Test Method for Major and Minor Elements in Coal NOTE 1—Segregation of Graded Sand—The graded standard sand
and Coke Ash By X-Ray Fluorescence should be handled in such a manner as to prevent segregation, since
2.2 ACI Document:3 variations in the grading of the sand cause variations in the consistency of
the mortar. In emptying bins or sacks, care should be exercised to prevent
ACI 201.2R Guide to Durable Concrete the formation of mounds of sand or craters in the sand, down the slopes
of which the coarser particles will roll. Bins should be of sufficient size to
3. Terminology permit these precautions. Devices for drawing the sand from bins by
3.1 Definitions of Terms Specific to This Standard: gravity should not be used.
3.1.1 composite sample—a sample that is constructed by 5.2 Hydrated Lime— The hydrated lime used in the tests
combining equal portions of grab or regular samples. shall be reagent-grade calcium hydroxide, 95 % minimum
3.1.2 established source—a source for which at least six calculated as Ca(OH)2(Note 2), and have a minimum fineness
months of continuous production quality assurance records of 2500 m2/kg as determined in accordance with Test Method
from a test frequency required for a new source are available, C 204.
sampled at the source.
NOTE 2—The calcium hydroxide should be protected from exposure to
3.1.3 grab sample—a sample that is taken in a single carbon dioxide. Material remaining in an opened container after a test
operation from a conveyor delivering to bulk storage, from should not be used for subsequent tests.
bags, or from a bulk shipment. Such a sample may, or may not,
reflect the composition or physical properties of a single lot of 5.3 Portland Cement— The portland cement used in the
fly ash or natural pozzolan. This type of sample can be used to Strength Activity Index with Portland Cement test shall comply
characterize small amounts of material. with the requirements of Specification C 150 and have a
3.1.4 jobsite or new source—a source for which less than minimum compressive strength of 35 MPa (5000 psi) at 28
six months of production records are available, sampled at the days and total alkalies (Na2O + 0.658 K 2O) not less than
source. 0.50 % nor more than 0.80 %.
3.1.5 lot—specific quantity of fly ash or natural pozzolan 5.3.1 The use of a locally available portland cement in the
offered for inspection at any one time. A lot may be one storage Strength Activity Index or a project cement that does not meet
bin or the contents of one or more transport units representing the requirements of the section on Materials is permitted when
material drawn from the same storage bin. the variations from the requirements of the section on Materials
3.1.6 regular sample—a sample that is constructed by are reported and when the use of such portland cement is
combining equal portions of grab samples that were taken at requested.
predetermined times or locations from any single lot of 6. Sample Type and Size
material.
6.1 Grab samples and regular samples shall have a mass of
4. Significance and Use at least 2 kg (4 lb).
6.2 Grab samples or regular samples taken at prescribed
4.1 These test methods are used to develop data for com- intervals over a period of time (see Table 1), may be combined
parison with the requirements of Specification C 618. These to form a composite sample representative of the fly ash or
test methods are based on standardized testing in the laboratory natural pozzolan produced during that period of time.
and are not intended to simulate job conditions. 6.3 Composite samples shall have a mass of at least 4 kg (8
4.1.1 Strength Activity Index—The test for strength activity lb).
index is used to determine whether fly ash or natural pozzolan 6.4 The sampling shall be done by, or under the direction of,
results in an acceptable level of strength development when a responsible representative of the purchaser.
used with hydraulic cement in concrete. Since the test is
performed with mortar, the results may not provide a direct 7. Sampling Procedure
correlation of how the fly ash or natural pozzolan will 7.1 The fly ash or natural pozzolan may be sampled by any
contribute to strength in concrete. one of the following methods:
4.1.2 Chemical Tests— The chemical component determi- 7.1.1 From Bulk Storage at Point of Discharge or from Rail
nations and the limits placed on each do not predict the Cars and Road Tankers—A sample may be taken by siphon
performance of a fly ash or natural pozzolan with hydraulic
cement in concrete, but collectively help describe composition
and uniformity of the material. TABLE 1 Minimum Sampling and Testing FrequencyA
Jobsite or New Established
Test Sample Type
SourceB SourceB
5. Materials
Moisture content Regular Daily or each Daily or each
5.1 Graded Standard Sand—The sand used for making test Loss on ignition 90 Mgc 360 MgC
specimens for the activity index with lime or portland cement Fineness (100 Tons) (400 Tons)
Density and the other Composite Monthly or each Monthly or each
shall be natural silica sand conforming to the requirements for tests in Specification 1 800 MgC (2 000 2 900 MgC
graded standard sand in Specification C 778. C 618, Tables 1 and 2 Tons) (3 200 Tons)
A
It should be noted that the minimum test frequency given in Table 1 is not
necessarily the frequency needed for quality control programs on some fly ash or
natural pozzolans.
3 B
Available from American Concrete Institute (ACI), P.O. Box 9094, Farmington For definitions, refer to the Terminology section.
C
Hills, MI 48333. Whichever comes first.
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C 311 – 05
tube during loading or by sampling tube from each loaded car Moisture content, %5~A/B!3100 (1)
or tanker. If the load is sampled at the point of discharge into
the rail car or tanker, the top surface shall be removed to a where:
A = mass loss during drying, and
depth of at least 200 mm (8 in.) before sampling. The sample
B = mass as received.
shall be identified with at least the date and shipment number.
7.1.2 From Bags in Storage—The regular sample shall LOSS ON IGNITION
comprise increments of equal size taken by sampling tube from
three bags selected at random from one lot of bagged material. 13. Procedure
The sample shall be identified with date and lot number. 13.1 Determine loss on ignition in accordance with the
7.1.3 From Conveyor Delivering to Bulk Storage—Take procedures outlined in Test Methods C 114, except that the
one sample of 2 kg (4 lb) or more of the material passing over material remaining from the determination of moisture content
the conveyor. This may be secured by taking the entire test shall be ignited to constant mass in an uncovered porcelain, not
sample in a single operation, known as the grab sample platinum, crucible at 750 6 50 °C (1382 6 190 °F).
method, or by combining several equal portions taken at
regular intervals, known as the regular sample method. Auto- 14. Calculation
matic samplers may be used to obtain samples. 14.1 Calculate the percentage of loss on ignition to the
7.2 Samples shall be treated as described in Section 8. nearest 0.1, as follows:

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NOTE 3—Some methods of loading or delivery of fly ash or natural Loss on ignition, %5~A/B!3100 (2)
pozzolan, particularly from an airstream or conveyor belt, may create
stratification or segregation in the material stream. Sampling techniques where:
must be designed to ensure that the sample is representative of the material A = loss in mass between 105 and 750 °C (221 and 1382
shipped. °F),
B = mass of moisture-free sample used.
8. Preparation and Storage of Samples
8.1 Prepare composite samples for the tests required in SILICON DIOXIDE, ALUMINUM OXIDE, IRON OXIDE,
Section 9, by arranging all grab or regular samples into groups CALCIUM OXIDE, MAGNESIUM OXIDE, SULFUR
covering the period or quantity to be represented by the TRIOXIDE, SODIUM OXIDE AND POTASSIUM OXIDE
sample. Take equal portions from each, sufficient to produce a
15. Procedure
composite sample large enough for the tests required. Mix the
composite sample thoroughly. 15.1 Determine the percentages of these oxides as required
8.2 Samples shall be stored in clean, airtight containers in accordance with the applicable sections of Test Methods
identified with the source and lot or period of time represented. C 114 for materials having an insoluble residue greater than
Untested portions of the sample shall be retained for at least 1 % (Note 4). Analysts performing sodium oxide and potas-
one month after all test results have been reported. sium oxide determinations shall observe the precautions out-
lined in the applicable section of Performance Specification
9. Testing Frequency C 1157 (refer to the section on Test Methods). Most pozzolans
9.1 General—When required, the purchaser shall specify dissolve completely in lithium borate fluxes.
the amount of testing for available alkalies, reactivity with NOTE 4—Rapid and instrumental methods may be employed similar to
cement alkalies, drying shrinkage, and air-entrainment. Make those in Test Methods C 114 and D 4326.
all other tests on regular or composite samples chosen as
specified in Table 1. AVAILABLE ALKALI

CHEMICAL ANALYSIS 16. Procedure


16.1 Weigh 5.0 g of the sample and 2.0 g of hydrated lime
10. General on a piece of weighing paper, carefully mix using a metal
10.1 All apparatus, reagents and techniques shall comply spatula, and transfer to a small plastic vial of approximately
with the requirements of Test Methods C 114. 25-mL capacity. Add 10.0 mL of water to this mixture, seal the
10.2 Purity of Water— Unless otherwise indicated, refer- vial by securing the cap or lid to the vial with tape (Note 5),
ences to water shall be understood to mean distilled water or blend by shaking until the mixture is uniform, and store at
water of equal purity. 38 6 2 °C.
MOISTURE CONTENT NOTE 5—To ensure that moisture loss from the paste does not occur,
place the sealed vial in a sealable container (such as a small sample or
11. Procedure mason jar), add sufficient water to cover the bottom of the container, and
seal.
11.1 Dry a weighed sample, as received, to constant weight
in an oven at 105 to 110 °C (221 to 230 °F). 16.2 Open the vial at the age of 28 days and transfer the
contents to a 250-mL casserole. Break up and grind the cake
12. Calculation with a pestle, adding a small amount of water, if necessary, so
12.1 Calculate the percentage of moisture to the nearest that a uniform slurry containing no lumps is obtained (Note 6).
0.1 %, as follows: Add sufficient water to make the total volume 200 mL. Let

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C 311 – 05
stand 1 h at room temperature with frequent stirring. Filter PHYSICAL TESTS
through a medium-textured filter paper onto a 500-mL volu-
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metric flask. Wash thoroughly with hot water (eight to ten DENSITY
times).
19. Procedure
NOTE 6—At times it may be necessary to break the vial and peel off the
plastic from the solid cake. In such cases, care should be exercised to 19.1 Determine the density of the sample in accordance
avoid the loss of material and to remove all solid material from the with the procedure described in Test Method C 188, except use
fragments of the vial. If the cake is too hard to break up and grind in the about 50 g of fly ash or natural pozzolan instead of approxi-
casserole, a mortar should be used. mately 64 g of cement as recommended in Test Method C 188.
16.3 Neutralize the filtrate with dilute HCl (1 + 3), using 1
FINENESS, AMOUNT RETAINED WHEN WET-SIEVED ON
to 2 drops of phenolphthalein solution as the indicator. Add
A 45-µm (NO. 325) SIEVE
exactly 5 mL of dilute HCl (1 + 3) in excess. Cool the solution
to room temperature and fill the flask to the mark with distilled
20. Procedure
water. Determine the amount of sodium and potassium oxides
in the solution using the flame photometric procedure, de- 20.1 Determine the amount of the sample retained when
scribed in Test Methods C 114, except that the standard wet-sieved on a 45-µm (No. 325) sieve, in accordance with
solutions shall be made up to contain 8 mL of calcium chloride Test Method C 430, with the following exceptions.
(CaCl2) stock solution per litre of standard solution, and the 20.1.1 Calibrate the 45-µm (No. 325) sieve using a cement
standard (SRM 114). Calculate the sieve correction factors as
solution as prepared shall be used in place of the solution of
follows:
cement.
CF5std2obs (5)
NOTE 7—The standard solutions made up with 8 mL of calcium
chloride (CaCl2) stock solution contain the equivalent of 504 ppm of CaO. where:
Tests have shown that this amount closely approximates the amount of CF = the sieve correction factor, %, (include a negative
calcium dissolved in the test solution. sign when appropriate),
std = the certified residue value for the SRM, %, and
17. Calculation and Report obs = the observed residue value for the SRM, %.
17.1 Calculate the results as weight percent of the original 20.1.2 Calculate the fineness of the fly ash or natural
pozzolan to the nearest 0.1 % as follows:
sample material. Report as equivalent percentage of sodium
oxide (Na2O), calculated as follows: RC5RS1CF (6)

Equivalent Na 2O, % 5 Na2O, %10.658 3 K2O, % (3) where:


RC = corrected sieve residue, %,
AMMONIA RS = observed residue for the test sample, %, and
CF = the sieve correction factor, %.
18. Procedure If the residue retained for the test sample is equal to zero
(RS = 0), then the sieve correction factor shall not be added to
18.1 Weigh 1.00 g of the fly ash sample into a 125 mL the test result to calculate the corrected sieve residue. In such
Erlenmeyer flask. Add 100 mL of ammonia-free water. Place a cases, the corrected fineness shall be reported as zero.
neoprene rubber stopper on the flask and swirl the contents to
thoroughly mix the sample and the water. NOTE 8—Test Method C 430 has been adopted for testing fly ash
fineness. However, certain requirements, such as cleaning of sieves and
18.2 Filter the mixture using a medium-textured filter paper interpretation of the test results, are sometimes not appropriate for fly
and save the filtrate for the ammonia determination. ashes.
18.3 Determine the concentration of ammonia in the filtrate
in accordance with the procedures outlined in Test Methods INCREASE OF DRYING SHRINKAGE OF MORTAR BARS
D 1426, Method A–Direct Nesslerization or Method B–Selec-
tive Ion Electrode. 21. Test Specimen
18.4 Calculate the ammonia concentration of the fly ash as 21.1 Prepare test specimens in accordance with the proce-
follows: dures described in Test Method C 157/C 157M, except mold
three mortar bars from both the control mix and the test mix
Ammonia, mg/kg 5 NW 3 VW/Wfa (4)
using the following proportions:

where: Control Mix Test Mix


NW = ammonia concentration of the water extract deter- Portland cement, g 500 500
Fly ash or natural None 125
mined by Test Methods D 1426, mg/L, pozzolan, g
VW = volume of water used for extracting ammonia from Graded standard sand, g 1375 1250
the fly ash sample, mL, and Water sufficient to produce a flow of 100 to 115 %
Wfa = Mass of fly ash sample used in the test, g.

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C 311 – 05
22. Procedure Test Mix
Portland cement, g 300
22.1 Cure and measure the test specimens in accordance Fly ash or natural pozzolan 75
with Test Method C 157/C 157M, except that the moist-curing 20–30 standard sand, g 1125
Water, mL, sufficient to give a flow of 80 to 95 Y
period (including the period in the molds) shall be 7 days, and Neutralized Vinsol resin solution, mL,A sufficient Z
the comparator reading at the age of 24 6 1⁄2 h shall be omitted. to produce an air content of 18 6 3 %
Immediately after taking the comparator reading at the end of
the 7-day moist-curing period, store the specimens in accor- A
The amount of Vinsol resin solution used shall be considered as part of the
mixing water.
dance with Test Method C 157/C 157M, and after 28 days of
air storage, take a comparator reading for the specimens in
accordance with Test Method C 157/C 157M. 25.2 The neutralized Vinsol resin solution used in this
section on Air-Entrainment of Mortar shall be either a com-
23. Calculation and Report mercial neutralized Vinsol resin solution or a neutralized
Vinsol resin solution prepared in accordance with Specification
23.1 Calculate the increase in drying shrinkage of the C 226. If it is necessary to dilute either of these solutions, use
mortar bars, Si, as follows: distilled or demineralized water. (Note 9.)
Si5St2Sc (7) NOTE 9—Dissolved minerals in drinking water may precipitate Vinsol
resin solutions and greatly diminish its air-entraining characteristics.
where:
St = average drying shrinkage of the test specimens calcu- 25.3 Prepare two test mixtures with sufficient neutralized
lated as follows, and Vinsol resin to produce an air content of 15 to 18 % in the first
Sc = average drying shrinkage of the control specimens mix and 18 to 21 % in the second mix. Then, determine by
calculated as follows: interpolation the amount of Vinsol resin, expressed as weight
@initial CRD 2 CRD# 3 100
percent of the cement, required to produce an air content of
S5 G (8) 18 %.

where: 26. Calculation


S = drying shrinkage of test or control speci- 26.1 Calculate the air content of the test mixtures as
mens, %, follows:
initial CRD = difference between the comparator reading Air content, volume %5100[12~Wa/W c!# (9)
of the specimen and the reference bar at 7
Wa5W/400 (10)
days of moist curing,
CRD = difference between the comparator reading 300111251751~300 3 P 3 0.01!
Wc5 (11)
of the specimen and the reference bar at 28
days of drying, and
FS D S D S D S
300 1125 75
3.15 1 2.65 1 D 1
300 3 P 3 0.01
1 DG
G = the gage length of the specimens 250 mm (10 where:
in.). Wa = actual weight per unit of volume of mortar as
23.2 Report the results to the nearest 0.01. If the average determined by Test Method C 185, g/mL,

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drying shrinkage of the control specimens is larger than the W = weight of the specified 400 mL of mortar (see Test
average drying shrinkage of the test specimens, prefix a minus Method C 185), g,
sign to the increase of drying shrinkage of mortar bars Wc = theoretical weight per unit of volume, calculated on
reported. an air-free basis and using the values for density and
quantities of the materials in the mix, g/mL,
SOUNDNESS P = percentage of mixing water plus Vinsol resin solution
based on weight of cement, and
24. Procedure D = density of fly ash or natural pozzolan in the mixture,
Mg/m3.
24.1 Conduct the soundness test in accordance with Test
Method C 151, except that the specimens shall be molded from STRENGTH ACTIVITY INDEX WITH PORTLAND CEMENT
a paste composed of 25 parts by weight of fly ash or natural 27. Specimens
pozzolan and 100 parts by weight of a portland cement
conforming to Specification C 150. 27.1 Mold the specimens from a control mixture and from a
test mixture in accordance with Test Method C 109/C 109M.
The portland cement used in the Strength Activity Index test
AIR-ENTRAINMENT OF MORTAR
shall comply with the requirements of Specification C 150 and
with the alkali and strength limits given in the section on
25. Procedure
Materials. In the test mixture, replace 20 % of the mass of the
25.1 Using portland cement conforming to the requirements amount of cement used in the control mixture by the same mass
for Type I or Type II of Specification C 150, prepare a test of the test sample. Make six-cube batches as follows:
mixture in accordance with Test Method C 185, using the 27.1.1 Control Mixture:
following proportions:

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500 g of portland cement Y = water required for the test mixture to be 65 of control
1375 g of graded standard sand flow.
242 mL of water
EFFECTIVENESS OF FLY ASH OR NATURAL POZZOLAN
27.1.2 Test Mixture: IN CONTROLLING ALKALI SILICA-REACTIONS (SEE
Appendix X1)
400 g of portland cement
100 g of test sample 32. Procedure
1375 g of graded standard sand
mL of water required for flow 6 5 of control mixture 32.1 Determine expansion of mortar made with a fly ash or
natural pozzolan and a test cement as a percent of expansion of
27.2 Number of Specimens: mortar made with low alkali cement in accordance with Test
27.2.1 Since Specification C 618 specifies that “meeting the Method C 441 as modified in the following paragraphs:
7 day or 28 day Strength Activity Index will indicate specifi- 32.1.1 Control Mixture— The control mixture will be made
cation compliance” only one age might be required. At the as required in Test Method C 441 except that the control
option of the producer or the user after preparing six-cube cement shall have an alkali content (as equivalent Na2O) less
batches, only three cubes of control and test mixtures need to than 0.60 % (Note 11).
be molded for either 7 or 28 day testing. NOTE 11—Generally, the control cement should have an alkali content
as equivalent Na2O between 0.50 and 0.60 %. However, lower alkali
28. Storage of Specimens control cement may be used, if desired, to demonstrate equivalence.
28.1 After molding, place the specimens and molds (on the 32.1.2 Test Mixture Using Fly Ash or Natural Pozzolan—
base plates) in the moist room or closet at 23.0 6 2.0 °C The combined quantity of cement plus fly ash or natural
(73.4 6 3 °F) for 20 to 24 h. While in the moist room or closet, pozzolan shall total 400 g (see Appendix X1). Use 900 g of
protect the surface from dripping water. Remove the molds borosilicate glass aggregate and sufficient mixing water to
from the moist room or closet and remove the cubes from the produce a flow between 100 and 115 % as determined in
molds. Place and store the cubes in saturated lime water as accordance with Test Method C 1437. The cement used in the
specified in Test Method C 109/C 109M. test mixture shall have an alkali content greater than that of the
NOTE 10—Take care to ensure against zones of stratification or pockets cement in the control mixture (Note 12).
of variation in temperature in the curing chamber. NOTE 12—Generally, this test cement will have an alkali content equal
to or higher than that used in the job.
29. Compressive Strength Test
32.1.3 Store and measure specimens as required in Test
29.1 Determine the compressive strength, as specified in
Method C 227. Measure length of specimens at ages of 1 and
Test Method C 109/C 109M, of three specimens of the control
14 days.
mixture and three specimens of the test mixture at ages of 7
days, or 28 days, or both, depending upon how many speci- 33. Report
mens were molded as prescribed in the section on Number of
33.1 Include in the report for each test mixture comparison
Specimens.
made:
30. Calculation 33.1.1 The 14 day expansion of the test mixture as a percent
of the control mixture at that age,
30.1 Calculate the strength activity index with portland
33.1.2 The identification and chemical analysis of the fly
cement as follows:
ash or natural pozzolan,
Strength activity index with portland cement =
33.1.3 The mass percentage of fly ash or natural pozzolan
(A/B) 3 100 (11)
based on the total mass of cement plus fly ash or natural
pozzolan in the test mixture, and
where: 33.1.4 The alkali content of control and test mixture ce-
A = average compressive strength of test mixture cubes, ments as equivalent alkali (Na2O + 0.658 K2O).
MPa (psi), and
B = average compressive strength of control mix cubes, EFFECTIVENESS OF FLY ASH OR NATURAL POZZOLAN
MPa (psi). IN CONTRIBUTING TO SULFATE RESISTANCE

34. Procedure
WATER REQUIREMENT 34.1 Compare the length change of mortar bars with abso-
lute expansion limits or compare the length change of mortar
31. Calculation bars made with a control cement with the length change of
31.1 Calculate the water requirement for the Strength Ac- mortar bars made with fly ash or natural pozzolan and a test
tivity Index with Portland Cement as follows: cement, in accordance with Test Method C 1012, as modified
Water requirement, percentage of control = in the following paragraphs. Results shall be evaluated using
(Y/242 3 100) (12) absolute limits (Procedure A) or the relative expansion limits
where: (Procedure B) in Specification C 618, Table 2A.

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C 311 – 05
34.2 Control Mixture for Procedure A—A control mixture is TABLE 2 Within and Between Lab Precision Estimates for C 114
not mandatory since performance measured using Procedure A Methods Applied to the Analysis of Fly AshA
is based on maximum expansion of the test mixture. If a 1s d2s
Oxide
control mixture is made for Procedure A then proportion it as W/L B/L W/L B/L
required in Test Method C 1012 using a cement meeting the SiO2 0.62 0.86 1.75 2.45
requirements of Specification C 150, Type II or Type V. Al2O3 1.46 2.29 4.12 6.48
Fe2O3
34.3 Test Mixture Using Fly Ash or Natural Pozzolan for <2 % 0.12 0.11 0.34 0.31
Procedure A—Make the combined quantity of cement plus fly $2 % 0.12 0.25 0.34 0.71
ash or natural pozzolan, by mass, the same as the total cement CaO 0.63 0.74 1.79 2.09
MgO 0.20 0.21 0.55 0.61
content of the control mixture described in the Making Mortars SO3 0.10 0.16 0.28 0.45
section of Test Method C 1012. The proportion of fly ash or Moisture 0.05 0.06 0.15 0.17
natural pozzolan may be varied using from 15 % to 50 %, by LOI 0.09 0.12 0.25 0.35
A
mass, of the total cement plus fly ash or natural pozzolan. Any The four values for SO3 were editorially corrected to reflect updated research
reports associated with this standard.
type of portland cement may be used to prepare test mixtures.
34.4 Control Mixture for Procedure B—Make the control
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mixture for Procedure B as required in Test Method C 1012 PRECISION AND BIAS
with the cement that is proposed for use in the project or a
36. Precision and Bias
cement that through performance or definition (Specification
C 150, Section 1) is expected to give satisfactory results (or a 36.1 Strength Activity Index Test:
cement for which the contribution to sulfate resistance is 36.1.1 Precision was determined from two interlaboratory
known and is satisfactory). studies involving two Class C fly ashes, two Class F fly ashes,
and one Class N pozzolan. Participating laboratories numbered
NOTE 13—The control cement should be chosen to give sulfate resis- 12 and 7 in the two studies.4
tance for the expected level of sulfate exposure. Experience has shown
36.1.2 The single-operator standard deviation for the
that Type II cements are often used for moderate levels of exposure. Type
V cement is commonly used for severe exposures (see X2.2 of Appendix Strength Activity Index test has been found to be 3.7 % (1s).
X2). This does not appear to vary either with material or with test
age, over the range of 7 to 28 days. Therefore, results of two
34.5 Test Mixture for Using Fly Ash or Natural Pozzolan for properly conducted tests by the same operator on the same
Procedure B—Make the combined quantity of cement plus fly material should not differ by more than 10.5 % (d2s) of the
ash or natural pozzolan, by mass, the same as the total cement average of the two results.
used in the control mixture. The proportion of fly ash or natural 36.1.3 The multilaboratory standard deviation for the
pozzolan may be varied from 15 % to 50 % of the total cement Strength Activity Index test has been found to be 4.5 % (1s).
plus fly ash or natural pozzolan by mass. Any type of portland This does not appear to vary either with material or with test
cement may be used to prepare test mixtures. age, over the range of 7 to 28 days. Therefore, results of two
34.6 For either Procedure A or B, store and measure properly conducted tests in different laboratories on the same
specimens as required in Test Method C 1012 for at least 6 material should not differ by more than 12.7 % (d2s) of the
months. average of the two results.
NOTE 14—Evaluation of the sulfate resistance of cementitious materials
36.1.4 Since there is no accepted reference material suitable
for use in certain situations or critical structures may require longer for determining the bias for this procedure, no statement on
periods of storage and additional length measurements. Refer to Test bias is being made.
Method C 1012 for guidance on this matter. 36.2 Chemical Analysis:
36.2.1 Precision and bias estimates for the test methods in
35. Report C 114 when applied to the analysis of pozzolans were calcu-
35.1 In addition to the information required in Test Method lated from an interlaboratory study involving 7 laboratories
C 1012, report the following information for each mixture each analyzing 4 NIST SRM fly ashes. A research report
comparison made: describing the results of this study is available from ASTM.5
35.2 For Procedure A, the age and expansion as a specific 36.2.2 Precision—Within-laboratory (W/L) and between-
amount, laboratory (B/L) estimates of standard deviation and estimates
of maximum differences expected between duplicate determi-
35.3 For Procedure B, the age and expansion as a percent of
nations in 95 % of comparisons6 are summarized in Table 2.
the control mixture at that age,
36.2.3 Bias—Statistically significant bias was found in the
35.4 The identification and chemical analysis including C3A determination of CaO and MgO. CaO determinations averaged
content of the cements used in both the control and test
mixtures,
35.5 The identification and chemical analysis of the fly ash 4
Supporting data have been filed at ASTM International Headquarters and may
or natural pozzolan used in the test mixtures, be obtained by requesting Research Report RR: C09-1001.
5
Supporting data have been filed at ASTM International Headquarters and may
35.6 The mass percentages of the fly ash or natural pozzolan
be obtained by requesting Research Report RR: C09-1008.
based on the total mass of cement plus fly ash or natural 6
These values represent, respectively, the (1s) and (d2s) limits as described in
pozzolan in the test mixture. Practice C 670.

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C 311 – 05
0.46 % higher than the value certified for the SRM. MgO has been found to be 7.4 % (1s %). The reproducibility of this
determinations averaged 0.19 % higher than the value certified test method is being determined and will be available on or
for the SRM. before July 2010.
36.3 Ammonia: 36.3.3 Bias—Since there is no accepted reference material
36.3.1 Precision of Method A (Direct Nesslerization) – The suitable for determining the bias for these procedures, no
single-laboratory coefficient of variation (repeatability) has statement on bias is being made.
been found to be 9.2 % (1s %). The reproducibility of this test
method is being determined and will be available on or before
37. Keywords
July 2010.
36.3.2 Precision of Method B (Selective Ion Electrode) – 37.1 fly ash; natural pozzolan
The single-laboratory coefficient of variation (repeatability)

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APPENDIXES

(Nonmandatory Information)

X1. COMMENTARY ON SECTION 32

X1.1 Test procedures in Section 32 are designed to deter- delineate any increase in expansion. The fly ash or natural
mine the effectiveness of fly ash, or natural pozzolan, in pozzolan percentage used may need to be sufficiently high to
preventing excessive expansion resulting from a reaction demonstrate that the percentage exceeds the pessimum if such
between certain aggregates and alkalies in portland-cement pessimum exists for the combination.
mixtures. Tests are made in accordance with Test Method
C 441 using: X1.6 Selection of the Low Alkali Control Cement—The test
procedure in this test method and requirements in Specification
X1.1.1 400 g of portland cement or a combined total of
C 618 are designed to measure the relative effectiveness of the
cement plus fly ash or natural pozzolan of 400 g,
fly ash or natural pozzolan in reducing expansion due to
X1.1.2 900 g of borosilicate glass, and
alkali-silica reactions. The effectiveness is a function of both
X1.1.3 Sufficient water to obtain a flow of 100 to 115 %.
the alkali content of the cement used in the test mixture and the
X1.2 The control mixture is made with a low-alkali percentage of fly ash or natural pozzolan. The higher the alkali
portland cement. The test mixture, made of a test percentage of content of the test mixture cement and the lower the percentage
the fly ash or natural pozzolan, can be made with the same of fly ash or natural pozzolan used, the more effective the fly
cement or any other cement having an equivalent alkali content ash or natural pozzolan. This test procedure and the 100 %
greater than 0.60 %. criterion of Specification C 618 can be used as a guide to
enhance field performance of job mixtures if it is assumed that
X1.3 Interpretation of Results—The fly ash or natural use of the low alkali control cement will prevent excessive
pozzolan should be considered “effective” when used at expansion in service with materials proposed for use in the job.
percentages equal to or greater than the percentages used in the This is the situation when the aggregates proposed for use
test mixture with cements having alkali contents that do not contain rapidly reactive constituents but do not exceed 0.05 %
exceed by more than 0.05 percentage points the alkali content expansion in three months or 0.10 % expansion in six months
of the cement used in the test mixture. when tested with the control cement in Test Method C 227. In
such instances the control cement used in this test method
X1.4 Selection of the Percentage of Fly Ash or Natural should have an alkali content as required to control the
Pozzolan—It may be necessary to make test mixtures with expansive reactions of the aggregates being used, for example
several percentages of fly ash or natural pozzolan to determine in the 0.50 to 0.60 % range. See the appendix to Specification
the minimum amount necessary to be considered “effective” in C 33.
reducing expansion to the level produced by the “control”
low-alkali cement. The minimum amount of fly ash or natural X1.6.1 Certain reactive aggregates have been identified
pozzolan should be 15 % by weight of cementitious material. which produce deleterious expansion after many years of
service when used with cements with equivalent alkali contents
X1.5 Selection of the Alkali Content of the Cement Used in well below 0.60 %. Often these reactive aggregates do not
the Test Mixture—In some instances it may not be necessary to produce expansions in Test Method C 227 exceeding those
demonstrate that the fly ash or natural pozzolan will reduce discussed in the appendix of Specification C 33 until a much
expansion, but rather that it will not increase expansion. In this later age, perhaps one or two years. In such instances the use
instance the test and control mixtures should be made with the of a control cement with an alkali content significantly less
same low alkali cement used in the control mixture to better than 0.60 % is appropriate.

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X2. COMMENTARY ON SECTION 34

X2.1 The test procedures in Section 34 are designed to addition of fly ash or natural pozzolan influences sulfate
evaluate the performance of particular fly ashes or natural resistance. However, as referenced in Test Method C 1012,
pozzolans in contributing to the resistance or durability of research has indicated that mortars meeting the expansion
concrete in a sulfate environment. Tests are made on mortars in criteria will perform adequately. Under Procedure B, the fly ash
accordance with Test Method C 1012. or natural pozzolan will be considered to be able to contribute
to sulfate resistance if the expansion of the test mixture does
X2.2 The control mixture should be made with a cement
not exceed that of the control mixture at an exposure time of at
that by performance or definition (Specification C 150, Section
least 6 months. It is recommended that the proportion of fly ash
1.1) is expected to give satisfactory results for the anticipated
or natural pozzolan used in the test mixture be the same one
level of sulfate exposure. ACI 201.2R recommends Type II
proposed for use in the project 6 2 %, and that the C3A content
cement when the sulfate content, expressed as SO4, is 0.10 to
of the project cement be equal to, or less than, that which was
0.20 percent in soils or 150 to 1500 ppm in waters. ACI 201.2R
used in the test mixtures. See Appendix X1, Technical Back-
recommends Type V cements when the sulfate content, ex-
ground, Test Method C 1012.
pressed as SO4, is 0.20 to 2.0 % in soils, or 1500 to 10 000 ppm
in waters. The test mixtures for both procedures may be made
with varying percentages of fly ash or natural pozzolan. Test X2.4 Selection of the Percentage of Fly Ash or Natural
mixtures can use cements with equal or higher or lower C3A Pozzolan—It may be necessary to make test mixtures with
contents that might not have given satisfactory results when several percentages of fly ash or natural pozzolan to determine
used alone. the amount necessary to obtain adequate resistance to different
concentrations of sulfates. Percentages used in a project should
X2.3 Interpretation of Results—The absolute expansion be within 2 % of those that are successful in the test mixtures
limits used in Procedure A make it difficult to ascertain how the or should be between two percentages that are successful.

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